Process of producing potassium ferrocyanide, potassium cyanide, potassium carbonate, and related products



'soLoMoN WEINBERQYIOF.PHILADEBPEIA, ENNsYLVANIA, YAssIfGNoRQBYMSNE?" `ASSIGNMENTS, TO YTI-IE UNITED STATES WO RABO, AICORPORATION F ARIZONA,

oL. COMANY, oF DENVER, copa...

PROCESS 0F PRODUCING PoTAssUivI FERR()'Q YANID'E,`A PoTAssIUMQYNIDE, YIioTAs- Y :il sIUM CARBo-NATE, AND YiELaTED PitonUeirs. i Yj g,

Laoaaza.

No Drawing, animationen@ iviach i1, isis,l

To all whom t 'may onemi B e it known .that 1:,1'SoLoMoN VEiNBERG,

a vvcitizen. of 'the United States, residing at Philadelphia, in the lc :ounty of V.Philadelphia andy State of Pennsylvania, havein-V vented a certain new ,and useful Process Vfor Producing. Potassium Ferrocyanide, Potassium Cyanide, Potassium Carbonate, and

i Related Products, of which the following. is

plates an improved',.utilizationof raw lvviool for the extraction fromsuclimaterial afvalliable ,by-products Yamong whichthe In bovenamed materials are included. l. The ,basis of the conception and develop#V mentotthe invention .requires for its .un-

derstanding'jr a brief consider ation 1of the or? dinary commercial .production oi potassium ferro-cyanide vand similar' products, vand l also the ordinary commercial treatment of raw Wool for obtaining `from it its contained extraneous matters, comprising animal fats,

Y moved from the Wool@ 'These" materials, lflOWfWellY are mllQh .dilated bi1. threlfaiively large amount `;of water required for'w'vashing,

suint, nitrogenous compounds,.e`tc. Potassium ferro-cyanide is ordinarily.

produced by combining potassium -carbonate with nitrogenous organic matter, such as horn, hair, blood, leather scraps, etc., and iron fragments. The potassium carbonate is heated in a furnace and the other materials are added in suitable proportionsand at suitable intervals, producing a violent reactionf. The resulting materialgis cooled, broken up, digested AWith vvaten and '.th efpoi tassium fierro-cyanide developed in the reaction is thus extracted. This process is .relatively too uncertain, expensive and in- 4`0` efficient, since the amount of organic matter to be added can never be accurately deterf mined in advance; the quantities of materials added are therefore never exact and usually only a small part of the theoretically available. product is obtained.y

The entire amount ofv nitrogenous carbon compounds is, in this'process, added in Vthe form o fhorn, hair, etc.1,as above enumerated.

vl/Vhile this provides theoretically all Vthe necessary amounts of' act-11.211,5" they' areirltgsomblin game matteradded in Such a,

liels, ingredients, yet

speeiacationof Lettesrat'em. Patented @in the. 0I@- Y ay thatgthey readily combine With v the ironandgthe potass ium carbonate. tion mustfbefrelatively long continuechthe Organic. matterY behgadded frm .time t9'- los@ by wlaiiizaioa ha?? tObG medal@ thfrriixtue at different per1ods of the reactionlto determine yvhatits condition is allies I Iearly' a s,possible, hovv muchlaolsorsahc metter 'SlhQulld :Ible addedf The practicall result. o these diiiicultiesA isi that the"reaction as a riilQmC-Llllnot AbeY c ontinued longenoughto get out any large pro-1 p ortiono'f the theoretically available PQtas,

slum'l'ferro-cyanide. l 20% of the.; amount Y' f theroretically available vfrom the base inay .terials may be takenas a liberalaverage.v

Rawwvool. has usually-been vv a shed `,i1 i a solution contain-ing cleaning; elements and the fresultingfluid containsthe nitrogenous and vfurthen modified bylthefwashingimater1als,.as, for example, the stated materials. iy

yare Sapolledfbysoaps and allral'ies jgener'f ally lused for Washingft fhas beenfrecog; f

nizedV that the'gmaterial thus y'obtained from Wool fis theoretically available forfthe production of potassium Y ferro-cyanidepbut the treatment. of the product on `a commercialthe stated .conditionsto such an extent that Following the conception .that potasf.-

Stated materials-from W010i' by-lpl'raducts has Y done.l Withy relatively glowlcost,i yieldinglmae terialA ,of ylarge value finy relation to vthe amount offbasicmaefial.treated andaieid i Y ing the diiiculties involved in the ordinary production of potassium ferro-cyanide as above briefly described, and also avoiding diiiicultiesencountered if it is attempted to deal Witi-ivool `Washings as also briefly Lde- Scrbd f.

In carrying out my invention` l clean raw Wool by a dry process, for example, by treating it Withfpulveriz'ed, more vor less dehydrated, calcium sulphate. VVhenthe dirty Wool is properly manipulated in the presence Y otkthis material, substantially all of the extraneous material is discharged from the Wool along With the cleaning' medium, leave. ing the Wool in exceptionally clean, dry and l' of the valuable material has beenv lost by un- Water is added at any time, and no drastic due` leaching or evaporation, and no n' substantial part of the valuable material is lost by the following recited steps of'treatment, due to the fact that no'excess amount of heating is required to drive-.off excess Water, which would involve the loss of valuable materials by volatilization;

*To the stated extracted material is added i' distilled Water until the soluble parts oi the mass are completely dissolved. The solution then contains all ofthe nitrogenous carbonY and potassium compounds' desired for the Y. presentpurpose, the amount of Water being only suiiicient to maintain these'in solution.

Substantially all ofthe cleaning powder and other matter discharge from the Wool7 such as vegetable particles, etc., remain out ot' the solution and the solution isl drawn oil and treated by any suitable process of concentration until the material becomes anpasty mass. To insure the presence of an ample amount ot nitrogen and carbon a` certain amount of 'y dried blood, leather clippings, dsc., istlien added, say, one-half, more or less, of the' Weight oic 'the pasty material.V While the nitrogen and carbon contained in this added organic 'matter is not in' theibestv form 'for combination with the other Yelements present,

'f' as are the carbon and nitrogen contained in the matter extracted tromthe Wool, yet sut-` ficieiit of these elements yis added to insure the complete reaction for the production'of the intended amount of potassium ferrocyanide. Finely divided iron is then added and the material `is heated. rlhis heating is preferably done in a reverberatory furnace so that the material is in'direct'contact with incastri the flame and air is excluded. Then the material is allowed to cool, ischopped up into small masses and lixiviated with Water, in which all ot the potassium ferro-cyanide is soluble.l This'solution-is then heated until .it reaches the proper specific gravity and the potassium ferro-cyanide is-jthen separated by filtration from the remainder of the material and crystallized. f f lt has been iound'that the best results are usually obtained when it is attempted to extract substantially 50% of the theoretically available potassiumferro cyanide. The amount of iron added to the material is-calculated on this basis and reasonablevariations from the exact amount are immaterial, since'this would result only in slightly increasing or decreasing the amount ot potassium ferroecyanide produced. The object of adding iron calculated to produce only substantially 50% of the available potassium ferro-cyanide is that the reaction of the iron with the other materials is a relatively sloW one and at the temperaturesinvolved, if the process is continued too long, the potassium terro-cyanide already developed is'vola't'ilized and Wasted, and alsoa certain part of the nitrogen isf driven off inthe form of ammonia. Up to substantially 50% of the available amount the reaction proceeds With suiiicient speed to avoid substantially all loss oi" the potassium ferro-cyanide and nitrogen. To extract a larger amount of the available potassium ferro-cyanide the process is repeated in a second or even a third stage..

Going back to the preferred treatment in which substantially 50% of the available potassium ferro-cyanide Awas' produced, the remaining material isa solid mass vcontaining potassium carbonate, potassium cyanide, yand potassium chloride, together 'With otherV unimportant materials. Of the stated materials they potassium carbonate and potassium cyanide are relatively more important; rlhey are extracted in successive stages by suitable well known methods of solution and separation.

an example of the `commercial im` portance ot the process', it maybe stated that approximately of the Weight of the raw Wool'is obtained in the solution formed by adding'water to the materials extracted from the wool the dry treatment, and of this approxiu'iately one-hall' is pure potash salts; that is, about 320 lbs. to the ton-of wool,V` oi'tliese available potassium salts, by the 50% method above described, approximately 200 lbs. more or less'oi potassium ferro` cyanide is produced, having a value at this time of'approximately $286. A substantial amount of both potassium cyanide and potassium carbonate is also produced, bringing the total value ot the products up to about $350.'

is compared With the firstdescribed conimercial method of producing potassium theoreticallly available Y ferroecyanide, it may be pointed out that by'. tliat=iiiethod only about 20%of the potassium terrocyanide `is produced.

- The process is for convenience recapitu! lated as nfollows, with a somewhat more letailed descriptionof t-he'nature ofl thema- 'teri'als Vproducedin. the vsuccessive steps :.V

First. 'Raw 'Wool is treated .With a pulverized di-yi cleaning agent, such as calcium sulphate, and the cleaning agent with .its-

contained.. matters is wool, producing: l A ,y

A. v A. complex, pulverized, substantially dry, mixture .Y containingg cleaningl powder discharged from the which is" practically insoluble. in Water,

y v B7. Phenol particlesot vegetable. matter, which are also insoluble, and various soluble nitrogen and potassium =compounds`fmore particularly de scribed in paragraphfB hereafter. v.

Second. Water is 4added to the material A suiiicient to take in solution all the solublepartsof A. Y l

Third.V The solution is drawn off and concentrated, producing:

. Y B. A pasty mass containing nitrogenous Vcarbon and potassium salts. The contents ot this mixture maybe more particularly' vdescribedas Vfollows, omitting any minor substances that are not'iinportant for the present purpose: l

B1. Free carbonicacid.y

' B2. Ammoiiiam carbonate formed by theVV decomposition'of urea. p f

vB3. Potassium carbonate formed at the `expense of certain secretions by a peculiar fermentation.

B4. Volatile fatty acids,A including acetic acid, propionic acid, butyric acid, valerianic acid, and caproicacid.A

B5. Higher fatty acids, such as oenanthic acid, caproic acid, oleic acid, stearic acid and v some acids ot Wax, especially cerotic acid. These acids are-contained as potassium salts and are formed'by action of potassium carbonate on the acids. Y

B6. Fats in the'form ot emulsions.

as phenol bisulphonate of aotassium. y Y

B8. Ordinary lactic acid. l

B9. yBenzoic acid formed by the decom-A position of hippuric acid.

Yet

B1". Oxalic acid. B171. Succinic acid. B12. Uric acid. BUP. Amido acids;0'l col leucine t rosine.

.rn-.r .1y B14.v Coloring mattersanalooous to those h m of urine,Y Y *K Fourth. Organic nitro en carbon com- :o pounds, such as dried blood, leather clippings, etc., equal to one-half, more or less' (in specific performance Vof the process) i by Weight of the amount of the pasty ma-V tei'iahand finely divided iron calculated (in a specific performance of the process)v to produce approximately l50% voii fthe avail-V able :potassiumv ferro-cyanide, :are added VYProducing: l 1- -m Al mixture or" B,oiiganie matter and iron.

Fifth-'The' mixture C is heated, conveniently inl av reverberatory furnace, and Withdrawnat such time asv volatile parts .ot the mixturecoinmenceto be lost in. consid.` erable amount. -This produces:

'-D. AA):compoundcontaining potassium V`terro-cyanide, f potassiuml carbonate', f, potassium cyanide,` potassium chloride,.and other Eighth. The materialV F is treated suc cessive stages of solution and separation to separate out potassium carbonate, potassium cyanide, and potassium chloride, when that product is desired. f

The addition` of organic matter such as bone, leather, etc., is not strictly essential,

and without this addition in step Fourth above, a great improvement over previous processes-ot producing the potassium ferro;`

cyanide is'made; but a still greater advantage is gainedwhen a certain amount of such organic matter is added, as above explained.

Iclaimzv V of potassium'consisting in extracting soluble potassiumsalts and nitrogenous carbon com-H j pounds from raw Woolin al substantially dry condition, adding Water sufficient to form a solution, concentrating the solution, adding comminuted ironheating and subsequently extracting the potassium ferrocyanide.`

2. The processoffmaking ferro-cyanide of potassiumconsisting in extracting potasv l. The process of I making `ferro-cyanide'` j .i

siuni salts andi nitrogenousV carbon com-" pounds fromfrayv Wool in a substantially jdry condition, adding Water to produce a solujtion containing various potassium salts andv nitrogenous carbon compounds, concentrating the-sol-utiomadding comminuted iron,

heating and removing the ferro-'cyanide .of

potassium thusformedfby suitable steps of solution and separation.

Y 3. Theprocess of making ferro-cyanideof potassium consisting in extracting potassium salts, and nitrogenous carbon compounds from raiv Woolv in a substantially drycondition, adding water to produce a solution containing Various potassium salts and nitrogenous carbon compounds, concentrating the solution, adding comminuted iron andV organic matter, heating, and removing the. ferro-cyanide of potassium thus formed by suitable steps of solution and separation.

Il. The process of making ferro-cyanide of eotassium consisting in extracting potassum salts and nitrogenous carbon compounds from raw wool in a Ysubstantially dry condition, adding water to produce a solution containing various potassium salts and nitrog- @nous carbon compounds concentrating the solution, adding comminutecl iron and organic matter, heating, removing the errocyanide of potassium, and extracting thereafter by suitable steps other potassium salts.

5. rEhe process of extracting potassium compounds available in Wool or similar 'animal fiber, consisting in treating the. same with pulverized dry cleaningrmaterial, discharging the cleaning material withother extraneous matters from the Wool, separat.- ing soluble potassium salts from this discharged cleaning materialby solution, and extracting one or more of the potassium compounds from ythe solution.

6. The process of extracting potassium compounds available in Wool or similar animal fibre consisting in treating the same With 2 pulverized dry cleaning material, discharging the cleaning material along With/other extraneous matter from theV said organic matter, separating soluble l, potassium salts from this discharged cleaning material, eX- tracting one or more potassium compounds from the solution by concentrating,-adding comminuted iron thereto", heating, and eX- tracting the potassium ferro-cyanide so produced from the remainder of the material.

VSOLOMON WEINBERG, 

